Ansa group 4 metal bis ( mu -substituted) aluminum complexes

Inactive Publication Date: 2000-10-31
THE DOW CHEM CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, there is no known successful preparation of bis(.mu.-substi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example

Example 1

Reaction of (t-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitanium dimethyl with two equivalents of tris(pentafluorophenyl)aluminum ##STR9##

NMR reactions were carried out in J-Young NMR tubes or NMR tubes with good seals, and the samples were loaded into the NMR tubes in a glove box after mixing the above two reagents ((t-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitanium dimethyl and FAAL) in 0.7 mL of benzene-d.sub.6 in a 1:2 ratio (0.02 mmol scale). The mixture was allowed to react at room temperature for 20 min before the NMR spectra were recorded. An orange solution was observed and the NMR data are consistent with the structure shown in the above equation. This species has a half-life of about 2.5 h at room temperature.

Spectroscopic data for Me.sub.2 Si(.eta..sup.5 -Me.sub.4 C.sub.5)(t-BuN)Ti[(.mu.-Me)Al(C.sub.6 F.sub.5).sub.3 ].sub.2 are as folllows. .sup.1 H NMR (C6D.sub.6, 23.degree. C.): .delta. 1.61 (s, 6 H, C.sub.5 Me.sub.4), 1.49 (s, 6 H,...

Example

Example 2

Reaction of (t-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitanium dimethyl with two equivalents of tris(pentafluorophenyl)aluminum, 24 hour study ##STR10##

NMR reactions were carried out in J-Young NMR tubes or NMR tubes with good seals, and the samples were loaded into the NMR tubes in a glove box after mixing the above two reagents ((t-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitaniu m dimethyl and FAAL) in 0.7 mL of benzene-d.sub.6 in a 1:2 ratio (0.02 mmol scale). The mixture was allowed to react at room temperature and the reaction was monitored by NMR measurements. The initially formed bis(.mu.-methyl) species Me.sub.2 Si(.eta..sup.5 -Me.sub.4 C.sub.5)(t-BuN)Ti[(.mu.-Me)Al(C.sub.6 F.sub.5).sub.3 ].sub.2 was slowly converted over 24 hours in quantitative yield to two species Me.sub.2 Si(.eta..sup.5 -Me.sub.4 C.sub.5)(t-BuN)Ti(C.sub.6 F.sub.5)(.mu.-Me)Al(C.sub.6 F.sub.5).sub.3 and [(C.sub.6 F.sub.5).sub.2 AlMe].sub.2 shown in the above equation.

S...

Example

Example 3

Reaction of (n-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitanium dimethyl with two equivalents of tris(pentafluorophenyl)aluminum ##STR11## A. Preparation of N-n-butylamino(dimethyl)tetramethylcyclopentadienylsilane

To a solution of 7.06 g (32.9 mmol) of chloro(dimethyl)tetramethylcyclopentadienylsilane in about 100 mL of hexane was slowly added about 8.0 mL (5.9 g, 8.1 mmol) of n-butylamine. Voluminous precipitate formed immediately. The reaction mixture was stirred overnight, filtered, the solids were extracted with hexane, and the volatiles were removed from the combined filtrates to give a pale yellow liquid. Yield: 8.09 g, 97.8 percent.

.sup.1 H NMR (C.sub.6 D.sub.6): d 2.83 (s, 1H, NH), 2.63 (q, J=6.7 Hz, 2H, CH.sub.2), 1.99 (s, 6H, C.sub.5 Me.sub.4), 1.85 (s, 6H, C.sub.5 Me.sub.4), 1.25 (br m, 4H, CH.sub.2 CH.sub.2), 0.88 (t, J=6.9 Hz, 3H, CH.sub.3), 0.17 (s, 1H, SiCH), 0.01 (s, 6H, SiMe.sub.2). .sup.13 C (C.sub.6 D.sub.6): d 135.4, 132.8, 56.9, 42.1, 37.4...

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Abstract

Ansa bis( mu -substituted) Group 4 metal and aluminum compounds comprising a single Group 4 metal atom and two aluminum metal atoms corresponding to the formula: wherein: L' is a pi -bonded group, M is a Group 4 metal, J is nitrogen or phosphorus; Z is a divalent bridging group causing the complex to have an ansa structure, R' is an inert monovalent ligand; r is one or two; X independently each occurrence is a Lewis basic ligand group able to form a mu -bridging ligand group, and optionally the two X groups may be joined together, and A' independently each occurrence is an aluminum containing Lewis acid compound that forms an adduct with the metal complex by means of the mu -bridging groups, and optionally two A' groups may be joined together thereby forming a single difunctional Lewis acid containing compound, and a method of preparation comprising contacting a charge-neutral Group IV metal coordination complex having at least two Lewis basic groups with at least two molar equivalents of charge-neutral aluminum coordination complexes having Lewis acidic aluminum atoms such that at least two of the aluminum atoms of the aluminum coordination complexes bond to at least two of the Lewis basic groups of the Group IV coordination complex.

Description

BACKGROUND INFORMATIONThe present invention relates to compounds that are useful as catalysts or catalyst components. More particularly, the present invention relates to such compounds comprising two aluminum and one Group 4 metal atom that are particularly adapted for use in the coordination polymerization of unsaturated compounds. Such compounds are particularly advantageous for use in a polymerization process wherein at least one polymerizable monomer is combined under polymerization conditions with a catalyst or catalyst composition to form a polymeric product.It is previously known in the art to activate Ziegler-Natta polymerization catalysts, particularly such catalysts comprising Group 3-10 metal complexes containing delocalized .pi.-bonded ligand groups, one uses Lewis acids to form catalytically active derivatives of such Group 3-10 metal complexes. Examples of suitable Lewis acids include tris(perfluorophenyl)borane and tris(perfluorobiphenyl)borane. Examples of such proce...

Claims

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Application Information

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IPC IPC(8): C07F17/00C07F5/00C07F5/06C07F7/10C07F7/28C07F19/00C08F4/642C08F4/659C08F4/6592C08F10/00
CPCC07F5/066C07F17/00C08F10/00C08F4/65912C08F4/6592C08F4/65927C08F4/61912C08F4/65908Y10S526/943C08F210/16C08F210/14C08F2500/08C08F2500/12C08F2500/03
Inventor CHEN, EUGENE Y.KRUPER, JR., WILLIAM J.NICKIAS, PETER N.WILSON, DAVID R.
Owner THE DOW CHEM CO
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